Development and validation of a sensitive HPLC method for the determination of lisinopril in human plasma after derivatization with 4-fluoro-7-nitro-2,1,3-benzoxadiazole  

作　　者：Reza Ahmadkhaniha Noushin Rastkari Syed Husain Hashemi Mousavi Effat Souri 

机构地区：[1]Department of Human Ecology,School of Public Health,Tehran University of Medical Sciences [2]Center for Air Pollution Research (CAPR),Institute for Environmental Research (IER),Tehran University of Medical Sciences [3]Department of Chemistry,Faculty of Engineering,South Tehran Branch,Islamic Azad University [4]Department of Medicinal Chemistry,Faculty of Pharmacy and Pharmaceutical Sciences Research Center,Tehran University of Medical Sciences

出　　处：《Journal of Chinese Pharmaceutical Sciences》2018年第9期623-629,共7页中国药学（英文版）

基　　金：The part of a Pham D thesis supported by Tehran University of Medical Sciences(Grant No.23049-92-02-92)

摘　　要：In this study, we developed a simple and sensitive HPLC method for the determination of lisinopril in human plasma. The sample clean-up was carried out by solid-phase extraction(SPE) using a cation-exchange(Strata-SCX~?) extraction cartridge. After a pre-column derivatization with 4-fluoro-7-nitro-2,1,3-benzoxadiazole, the reaction mixture was analyzed on an Agilent Zorbax SB~?-C_(18)(150 mm×4.6 mm, 5 μm). The flow rate was set at 1.0 mL/min. Fluorescence detection was performed at an excitation wavelength of 470 nm and an emission wavelength of 530 nm. The mobile phase consisted of a mixture of methanol and 0.02 M sodium dihydrogen phosphate(pH = 3.0, 60:40, v/v). The average extraction recovery of lisinopril and fluvoxamine(internal standard) was >85%. The method exhibited a linear calibration curve over the concentration range of 1–1000 ng/mL with a correlation coefficient(r^2) of ≥0.98 and a limit of quantification(LOQ) equal to 2 ng/mL. The within-run and between-run precisions were satisfactory with an RSD of 3.8%–13.7%(accuracy: from 95.0% to 96.4%) and 4.273%–14.3%(accuracy: from 94.4% to 98.5%), respectively.In this study, we developed a simple and sensitive HPLC method for the determination of lisinopril in human plasma. The sample clean-up was carried out by solid-phase extraction(SPE) using a cation-exchange(Strata-SCX~?) extraction cartridge. After a pre-column derivatization with 4-fluoro-7-nitro-2,1,3-benzoxadiazole, the reaction mixture was analyzed on an Agilent Zorbax SB~?-C_(18)(150 mm×4.6 mm, 5 μm). The flow rate was set at 1.0 mL/min. Fluorescence detection was performed at an excitation wavelength of 470 nm and an emission wavelength of 530 nm. The mobile phase consisted of a mixture of methanol and 0.02 M sodium dihydrogen phosphate(pH = 3.0, 60:40, v/v). The average extraction recovery of lisinopril and fluvoxamine(internal standard) was >85%. The method exhibited a linear calibration curve over the concentration range of 1–1000 ng/mL with a correlation coefficient(r^2) of ≥0.98 and a limit of quantification(LOQ) equal to 2 ng/mL. The within-run and between-run precisions were satisfactory with an RSD of 3.8%–13.7%(accuracy: from 95.0% to 96.4%) and 4.273%–14.3%(accuracy: from 94.4% to 98.5%), respectively.

关 键 词：LISINOPRIL HPLC DERIVATIZATION 4-Fluoro-7-nitro-2 1 3 -benzoxadiazole 

分 类 号：R917[医药卫生—药物分析学]